# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1246 # (Title) X-ray crystal structures of nitridotechnetium(V) complexes of # propylene, butylene and pentylene amine oximes different in carbon chain # length data_TcN-BnAO(2) #------------------------------------------------------------------------------ _audit_creation_date 'Thu Oct 17 15:41:19 1996' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 733.66 _chemical_formula_analytical ? _chemical_formula_sum 'C38 H51 B N5 O3 Tc ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.683(3) _cell_length_b 24.944(6) _cell_length_c 15.149(2) _cell_angle_alpha 90 _cell_angle_beta 97.39(3) _cell_angle_gamma 90 _cell_volume 3628(1) _cell_formula_units_Z 4 _cell_measurement_temperature 286.2 _cell_measurement_reflns_used 19 _cell_measurement_theta_min 23.1 _cell_measurement_theta_max 28.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1544.00 _exptl_absorpt_coefficient_mu 3.529 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.696 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 286.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -9.30 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -6 4 -1 -4 3 -1 -3 4 _diffrn_reflns_number 6397 _reflns_number_total 6154 _reflns_number_observed 4211 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 4.62 _diffrn_reflns_av_sigmaI/netI 0.057 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 63.09 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04340 _diffrn_orient_matrix_UB_12 0.02028 _diffrn_orient_matrix_UB_13 0.04629 _diffrn_orient_matrix_UB_21 -0.09322 _diffrn_orient_matrix_UB_22 -0.01496 _diffrn_orient_matrix_UB_23 -0.02378 _diffrn_orient_matrix_UB_31 0.01648 _diffrn_orient_matrix_UB_32 -0.03117 _diffrn_orient_matrix_UB_33 0.04151 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Tc 0 4 0.006 3.005 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 152 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 12 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 20 0.031 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 204 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; B 0 4 0.009 0.004 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Tc1 0.28084(4) 0.03151(2) 0.89146(2) 0.04317(10) Uani d . 1.00 . O1 0.1587(3) -0.0207(1) 1.0392(2) 0.060(1) Uani d . 1.00 . O2 0.2158(4) 0.0766(1) 1.0669(2) 0.065(1) Uani d . 1.00 . O3 0.0308(3) 0.0532(1) 0.8561(2) 0.054(1) Uani d . 1.00 . N1 0.4457(4) 0.0214(1) 0.9086(3) 0.056(1) Uani d . 1.00 . N2 0.1989(4) -0.0307(2) 0.9578(2) 0.047(1) Uani d . 1.00 . N3 0.2594(4) 0.0896(2) 0.9858(2) 0.050(1) Uani d . 1.00 . N4 0.2384(4) -0.0285(1) 0.7903(2) 0.044(1) Uani d . 1.00 . N5 0.2852(4) 0.1060(1) 0.8209(2) 0.045(1) Uani d . 1.00 . C1 0.1873(5) -0.0769(2) 0.9239(3) 0.047(1) Uani d . 1.00 . C2 0.2912(5) 0.1381(2) 0.9737(3) 0.054(2) Uani d . 1.00 . C3 0.2408(5) -0.0839(2) 0.8343(3) 0.050(2) Uani d . 1.00 . C4 0.3388(5) 0.1506(2) 0.8836(3) 0.055(2) Uani d . 1.00 . C5 0.1330(7) -0.1236(2) 0.9710(4) 0.071(2) Uani d . 1.00 . C6 0.2898(7) 0.1804(2) 1.0424(4) 0.081(2) Uani d . 1.00 . C7 0.1523(7) -0.1226(2) 0.7733(4) 0.067(2) Uani d . 1.00 . C8 0.3905(6) -0.1048(2) 0.8532(4) 0.063(2) Uani d . 1.00 . C9 0.2837(7) 0.2044(2) 0.8468(4) 0.082(2) Uani d . 1.00 . C10 0.5001(6) 0.1507(2) 0.8943(4) 0.072(2) Uani d . 1.00 . C11 0.3270(6) -0.0255(2) 0.7155(3) 0.056(2) Uani d . 1.00 . C12 0.3404(6) 0.1032(2) 0.7331(4) 0.060(2) Uani d . 1.00 . C13 0.2796(6) 0.0146(2) 0.6442(3) 0.066(2) Uani d . 1.00 . C14 0.2442(6) 0.0704(2) 0.6679(3) 0.065(2) Uani d . 1.00 . C15 0.6688(5) 0.1282(2) 0.5125(3) 0.048(1) Uani d . 1.00 . C16 0.5662(5) 0.0887(2) 0.5041(3) 0.056(2) Uani d . 1.00 . C17 0.4585(5) 0.0878(2) 0.4343(4) 0.063(2) Uani d . 1.00 . C18 0.4484(6) 0.1264(2) 0.3705(3) 0.064(2) Uani d . 1.00 . C19 0.5468(6) 0.1658(2) 0.3751(3) 0.062(2) Uani d . 1.00 . C20 0.6549(6) 0.1660(2) 0.4444(4) 0.058(2) Uani d . 1.00 . C21 0.7289(5) 0.1785(2) 0.6681(3) 0.051(2) Uani d . 1.00 . C22 0.6124(6) 0.2102(2) 0.6448(4) 0.067(2) Uani d . 1.00 . C23 0.5742(8) 0.2506(2) 0.7005(5) 0.094(3) Uani d . 1.00 . C24 0.6498(9) 0.2596(3) 0.7819(5) 0.107(3) Uani d . 1.00 . C25 0.7606(8) 0.2285(3) 0.8076(4) 0.093(2) Uani d . 1.00 . C26 0.7987(6) 0.1874(2) 0.7532(4) 0.070(2) Uani d . 1.00 . C27 0.9332(5) 0.1562(2) 0.5688(3) 0.047(1) Uani d . 1.00 . C28 1.0164(6) 0.1963(2) 0.6128(3) 0.057(2) Uani d . 1.00 . C29 1.1431(6) 0.2124(2) 0.5854(4) 0.066(2) Uani d . 1.00 . C30 1.1889(6) 0.1887(2) 0.5138(4) 0.068(2) Uani d . 1.00 . C31 1.1101(6) 0.1500(2) 0.4672(3) 0.064(2) Uani d . 1.00 . C32 0.9843(5) 0.1349(2) 0.4942(3) 0.052(2) Uani d . 1.00 . C33 0.8068(5) 0.0763(2) 0.6488(3) 0.044(1) Uani d . 1.00 . C34 0.8879(5) 0.0350(2) 0.6189(3) 0.051(1) Uani d . 1.00 . C35 0.8940(6) -0.0162(2) 0.6546(3) 0.060(2) Uani d . 1.00 . C36 0.8176(6) -0.0294(2) 0.7220(4) 0.064(2) Uani d . 1.00 . C37 0.7363(6) 0.0091(2) 0.7535(3) 0.060(2) Uani d . 1.00 . C38 0.7321(5) 0.0603(2) 0.7176(3) 0.054(2) Uani d . 1.00 . B1 0.7854(6) 0.1344(2) 0.6008(3) 0.044(2) Uani d . 1.00 . H1 0.202(8) 0.039(3) 1.060(5) 0.2331 Uiso calc . 1.00 . H2 0.1372 -0.0319 0.7497 0.0798 Uiso calc . 1.00 . H3 0.1649 0.1098 0.8128 0.0798 Uiso calc . 1.00 . H4 0.163(6) -0.155(2) 0.956(3) 0.1026 Uiso calc . 1.00 . H5 0.158(6) -0.124(2) 1.030(3) 0.1055 Uiso calc . 1.00 . H6 0.043(6) -0.126(3) 0.960(4) 0.1468 Uiso calc . 1.00 . H7 0.350(6) 0.207(2) 1.039(4) 0.1252 Uiso calc . 1.00 . H8 0.207(5) 0.199(2) 1.033(3) 0.0921 Uiso calc . 1.00 . H9 0.298(6) 0.167(2) 1.103(3) 0.1041 Uiso calc . 1.00 . H10 0.055(5) -0.116(2) 0.769(3) 0.0734 Uiso calc . 1.00 . H11 0.162(5) -0.160(2) 0.797(3) 0.0757 Uiso calc . 1.00 . H12 0.178(5) -0.123(2) 0.714(3) 0.0814 Uiso calc . 1.00 . H13 0.451(6) -0.079(2) 0.885(3) 0.1065 Uiso calc . 1.00 . H14 0.394(5) -0.139(2) 0.886(3) 0.0903 Uiso calc . 1.00 . H15 0.423(5) -0.112(2) 0.794(3) 0.0789 Uiso calc . 1.00 . H16 0.175(5) 0.205(2) 0.848(3) 0.0907 Uiso calc . 1.00 . H17 0.338(6) 0.232(2) 0.887(3) 0.1154 Uiso calc . 1.00 . H18 0.299(6) 0.210(2) 0.786(4) 0.1228 Uiso calc . 1.00 . H19 0.541(5) 0.116(2) 0.918(3) 0.0887 Uiso calc . 1.00 . H20 0.530(5) 0.183(2) 0.940(3) 0.1041 Uiso calc . 1.00 . H21 0.537(5) 0.162(2) 0.842(3) 0.1033 Uiso calc . 1.00 . H22 0.323(4) -0.061(2) 0.686(3) 0.0660 Uiso calc . 1.00 . H23 0.420(5) -0.018(2) 0.742(3) 0.0700 Uiso calc . 1.00 . H24 0.349(4) 0.135(2) 0.714(3) 0.0524 Uiso calc . 1.00 . H25 0.435(5) 0.084(2) 0.737(3) 0.0761 Uiso calc . 1.00 . H26 0.360(4) 0.016(2) 0.609(3) 0.0671 Uiso calc . 1.00 . H27 0.214(6) -0.003(2) 0.595(4) 0.1390 Uiso calc . 1.00 . H28 0.227(5) 0.091(2) 0.614(3) 0.0786 Uiso calc . 1.00 . H29 0.155(6) 0.072(2) 0.691(4) 0.1199 Uiso calc . 1.00 . H30 -0.031(6) 0.050(2) 0.804(3) 0.1121 Uiso calc . 1.00 . H31 -0.013(4) 0.038(2) 0.899(3) 0.0536 Uiso calc . 1.00 . H32 0.575(4) 0.063(1) 0.546(2) 0.0459 Uiso calc . 1.00 . H33 0.397(5) 0.062(2) 0.435(3) 0.0843 Uiso calc . 1.00 . H34 0.376(4) 0.126(2) 0.320(3) 0.0587 Uiso calc . 1.00 . H35 0.542(4) 0.191(2) 0.330(3) 0.0570 Uiso calc . 1.00 . H36 0.718(4) 0.192(2) 0.449(3) 0.0582 Uiso calc . 1.00 . H37 0.566(4) 0.206(2) 0.590(2) 0.0462 Uiso calc . 1.00 . H38 0.507(6) 0.270(2) 0.675(4) 0.1284 Uiso calc . 1.00 . H39 0.620(6) 0.285(2) 0.818(4) 0.1234 Uiso calc . 1.00 . H40 0.821(5) 0.230(2) 0.866(3) 0.0777 Uiso calc . 1.00 . H41 0.877(4) 0.168(2) 0.773(3) 0.0595 Uiso calc . 1.00 . H42 0.990(4) 0.216(1) 0.661(2) 0.0467 Uiso calc . 1.00 . H43 1.182(5) 0.238(2) 0.619(3) 0.0712 Uiso calc . 1.00 . H44 1.269(5) 0.199(2) 0.495(3) 0.0840 Uiso calc . 1.00 . H45 1.138(5) 0.134(2) 0.411(3) 0.0813 Uiso calc . 1.00 . H46 0.927(4) 0.108(2) 0.459(3) 0.0694 Uiso calc . 1.00 . H47 0.938(4) 0.044(2) 0.568(2) 0.0551 Uiso calc . 1.00 . H48 0.942(4) -0.041(2) 0.627(3) 0.0557 Uiso calc . 1.00 . H49 0.817(4) -0.062(1) 0.748(2) 0.0436 Uiso calc . 1.00 . H50 0.690(5) 0.000(2) 0.793(3) 0.0870 Uiso calc . 1.00 . H51 0.684(4) 0.086(2) 0.739(3) 0.0636 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tc(1) 0.0402(2) 0.0467(2) 0.0428(2) -0.0027(2) 0.0064(2) 0.0029(2) O(1) 0.060(2) 0.072(2) 0.050(2) -0.011(2) 0.017(2) 0.002(2) O(2) 0.077(3) 0.071(2) 0.051(2) -0.005(2) 0.019(2) -0.001(2) O(3) 0.033(2) 0.064(2) 0.064(2) -0.009(2) 0.008(2) 0.004(2) N(1) 0.037(2) 0.046(3) 0.083(3) -0.005(2) -0.002(2) 0.000(2) N(2) 0.048(2) 0.050(2) 0.045(2) -0.001(2) 0.007(2) 0.003(2) N(3) 0.048(3) 0.053(3) 0.050(2) -0.009(2) 0.004(2) -0.004(2) N(4) 0.045(2) 0.045(2) 0.045(2) -0.002(2) 0.011(2) 0.002(2) N(5) 0.041(2) 0.048(2) 0.049(2) -0.003(2) 0.012(2) -0.006(2) C(1) 0.048(3) 0.044(3) 0.049(3) 0.002(3) 0.010(2) 0.010(2) C(2) 0.045(3) 0.054(3) 0.062(3) -0.004(3) 0.006(3) -0.012(3) C(3) 0.056(3) 0.048(3) 0.045(3) -0.001(3) 0.006(3) 0.005(2) C(4) 0.063(4) 0.043(3) 0.062(3) -0.008(3) 0.014(3) 0.002(3) C(5) 0.082(5) 0.055(3) 0.080(4) -0.010(4) 0.024(4) 0.016(3) C(6) 0.098(5) 0.064(4) 0.084(4) -0.008(4) 0.022(4) -0.023(3) C(7) 0.086(4) 0.048(3) 0.066(4) -0.009(4) 0.008(4) 0.002(3) C(8) 0.061(4) 0.058(4) 0.070(4) 0.012(3) 0.011(3) 0.012(3) C(9) 0.103(5) 0.053(4) 0.092(4) 0.001(4) 0.023(5) 0.002(3) C(10) 0.058(4) 0.075(4) 0.081(4) -0.023(3) 0.005(3) -0.004(3) C(11) 0.066(3) 0.049(3) 0.056(3) 0.009(3) 0.019(3) 0.003(3) C(12) 0.062(4) 0.059(4) 0.062(3) -0.005(3) 0.014(3) 0.019(3) C(13) 0.082(4) 0.062(4) 0.060(3) 0.008(3) 0.025(3) 0.011(3) C(14) 0.083(4) 0.066(4) 0.046(3) 0.000(4) 0.006(3) 0.004(3) C(15) 0.040(3) 0.046(3) 0.059(3) 0.006(3) 0.008(3) -0.005(2) C(16) 0.044(3) 0.063(3) 0.060(3) 0.002(3) 0.004(3) 0.002(3) C(17) 0.044(3) 0.078(4) 0.067(3) -0.006(3) 0.006(3) -0.007(3) C(18) 0.043(3) 0.088(4) 0.057(3) 0.010(3) -0.001(3) -0.010(3) C(19) 0.063(4) 0.063(4) 0.060(3) 0.009(3) 0.002(3) 0.006(3) C(20) 0.052(3) 0.051(3) 0.069(3) -0.004(3) 0.001(3) -0.004(3) C(21) 0.043(3) 0.053(3) 0.058(3) -0.011(3) 0.015(3) -0.005(3) C(22) 0.079(4) 0.051(3) 0.075(4) 0.005(3) 0.025(4) -0.002(3) C(23) 0.131(6) 0.055(4) 0.108(5) 0.021(4) 0.067(5) 0.009(4) C(24) 0.169(8) 0.059(4) 0.110(5) -0.016(5) 0.078(5) -0.024(4) C(25) 0.117(6) 0.090(5) 0.079(4) -0.052(4) 0.040(4) -0.032(4) C(26) 0.065(4) 0.077(4) 0.069(4) -0.021(3) 0.019(3) -0.018(3) C(27) 0.043(3) 0.048(3) 0.048(3) 0.000(3) 0.002(2) 0.000(2) C(28) 0.053(3) 0.056(3) 0.060(3) 0.000(3) 0.009(3) -0.004(3) C(29) 0.055(4) 0.060(4) 0.080(4) -0.012(3) 0.004(3) 0.007(3) C(30) 0.054(4) 0.076(4) 0.077(4) -0.004(3) 0.018(3) 0.021(3) C(31) 0.065(4) 0.070(4) 0.061(3) 0.000(3) 0.021(3) 0.008(3) C(32) 0.052(3) 0.052(3) 0.051(3) -0.002(3) 0.008(3) 0.004(2) C(33) 0.035(3) 0.052(3) 0.046(3) -0.004(2) 0.005(2) 0.000(2) C(34) 0.052(3) 0.050(3) 0.051(3) -0.004(3) 0.007(2) -0.003(3) C(35) 0.064(4) 0.051(4) 0.067(4) -0.004(3) 0.010(3) -0.009(3) C(36) 0.059(3) 0.058(3) 0.070(4) -0.016(4) -0.004(3) 0.007(3) C(37) 0.041(3) 0.075(4) 0.059(3) -0.014(3) -0.004(3) 0.014(3) C(38) 0.042(3) 0.061(4) 0.059(3) 0.001(3) 0.004(3) -0.004(3) B(1) 0.040(3) 0.049(3) 0.046(3) 0.001(3) 0.009(3) -0.008(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00004|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0014(3) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4211 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0461 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0416 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.168 _refine_ls_shift/esd_max 0.2310 _refine_ls_shift/esd_mean 0.0290 _refine_diff_density_min -0.85 _refine_diff_density_max 0.68 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tc(1) N(1) 1.604(4) 1_555 1_555 yes Tc(1) N(2) 2.062(4) 1_555 1_555 yes Tc(1) N(3) 2.064(4) 1_555 1_555 yes Tc(1) N(4) 2.144(3) 1_555 1_555 yes Tc(1) N(5) 2.146(4) 1_555 1_555 yes O(1) N(2) 1.362(4) 1_555 1_555 yes O(2) N(3) 1.387(4) 1_555 1_555 yes N(2) C(1) 1.262(5) 1_555 1_555 yes N(3) C(2) 1.269(5) 1_555 1_555 yes N(4) C(3) 1.533(5) 1_555 1_555 yes N(4) C(11) 1.508(6) 1_555 1_555 yes N(5) C(4) 1.511(6) 1_555 1_555 yes N(5) C(12) 1.498(6) 1_555 1_555 yes C(1) C(3) 1.523(6) 1_555 1_555 yes C(1) C(5) 1.496(7) 1_555 1_555 yes C(2) C(4) 1.528(6) 1_555 1_555 yes C(2) C(6) 1.483(7) 1_555 1_555 yes C(3) C(7) 1.523(7) 1_555 1_555 yes C(3) C(8) 1.533(7) 1_555 1_555 yes C(4) C(9) 1.521(7) 1_555 1_555 yes C(4) C(10) 1.549(7) 1_555 1_555 yes C(11) C(13) 1.500(7) 1_555 1_555 yes C(12) C(14) 1.510(7) 1_555 1_555 yes C(13) C(14) 1.488(7) 1_555 1_555 yes C(15) C(16) 1.393(6) 1_555 1_555 yes C(15) C(20) 1.392(6) 1_555 1_555 yes C(15) B(1) 1.644(7) 1_555 1_555 yes C(16) C(17) 1.387(7) 1_555 1_555 yes C(17) C(18) 1.359(7) 1_555 1_555 yes C(18) C(19) 1.364(7) 1_555 1_555 yes C(19) C(20) 1.383(7) 1_555 1_555 yes C(21) C(22) 1.385(7) 1_555 1_555 yes C(21) C(26) 1.395(7) 1_555 1_555 yes C(21) B(1) 1.640(7) 1_555 1_555 yes C(22) C(23) 1.394(8) 1_555 1_555 yes C(23) C(24) 1.369(9) 1_555 1_555 yes C(24) C(25) 1.340(10) 1_555 1_555 yes C(25) C(26) 1.395(8) 1_555 1_555 yes C(27) C(28) 1.397(6) 1_555 1_555 yes C(27) C(32) 1.397(6) 1_555 1_555 yes C(27) B(1) 1.660(7) 1_555 1_555 yes C(28) C(29) 1.403(7) 1_555 1_555 yes C(29) C(30) 1.359(7) 1_555 1_555 yes C(30) C(31) 1.367(7) 1_555 1_555 yes C(31) C(32) 1.386(7) 1_555 1_555 yes C(33) C(34) 1.404(6) 1_555 1_555 yes C(33) C(38) 1.401(6) 1_555 1_555 yes C(33) B(1) 1.624(7) 1_555 1_555 yes C(34) C(35) 1.384(6) 1_555 1_555 yes C(35) C(36) 1.376(7) 1_555 1_555 yes C(36) C(37) 1.366(7) 1_555 1_555 yes C(37) C(38) 1.388(7) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Tc(1) N(2) 103.9(2) 1_555 1_555 1_555 yes N(1) Tc(1) N(3) 100.7(2) 1_555 1_555 1_555 yes N(1) Tc(1) N(4) 95.8(2) 1_555 1_555 1_555 yes N(1) Tc(1) N(5) 97.7(2) 1_555 1_555 1_555 yes N(2) Tc(1) N(3) 96.4(2) 1_555 1_555 1_555 yes N(2) Tc(1) N(4) 76.9(1) 1_555 1_555 1_555 yes N(2) Tc(1) N(5) 158.0(1) 1_555 1_555 1_555 yes N(3) Tc(1) N(4) 163.3(1) 1_555 1_555 1_555 yes N(3) Tc(1) N(5) 75.4(1) 1_555 1_555 1_555 yes N(4) Tc(1) N(5) 105.2(1) 1_555 1_555 1_555 yes N(3) O(2) H(1) 100(5) 1_555 1_555 1_555 no H(30) O(3) H(31) 105(4) 1_555 1_555 1_555 no Tc(1) N(2) O(1) 118.4(3) 1_555 1_555 1_555 yes Tc(1) N(2) C(1) 120.6(3) 1_555 1_555 1_555 yes O(1) N(2) C(1) 121.0(4) 1_555 1_555 1_555 yes Tc(1) N(3) O(2) 121.2(3) 1_555 1_555 1_555 yes Tc(1) N(3) C(2) 121.4(3) 1_555 1_555 1_555 yes O(2) N(3) C(2) 117.3(4) 1_555 1_555 1_555 yes Tc(1) N(4) C(3) 109.1(2) 1_555 1_555 1_555 yes Tc(1) N(4) C(11) 115.2(3) 1_555 1_555 1_555 yes Tc(1) N(4) H(2) 122.2(3) 1_555 1_555 1_555 no C(3) N(4) C(11) 113.2(4) 1_555 1_555 1_555 yes C(3) N(4) H(2) 97.9(3) 1_555 1_555 1_555 no C(11) N(4) H(2) 97.9(3) 1_555 1_555 1_555 no Tc(1) N(5) C(4) 110.6(3) 1_555 1_555 1_555 yes Tc(1) N(5) C(12) 115.8(3) 1_555 1_555 1_555 yes Tc(1) N(5) H(3) 92.3(2) 1_555 1_555 1_555 no C(4) N(5) C(12) 117.3(4) 1_555 1_555 1_555 yes C(4) N(5) H(3) 105.4(3) 1_555 1_555 1_555 no C(12) N(5) H(3) 112.2(3) 1_555 1_555 1_555 no N(2) C(1) C(3) 116.4(4) 1_555 1_555 1_555 yes N(2) C(1) C(5) 122.3(4) 1_555 1_555 1_555 yes C(3) C(1) C(5) 121.1(4) 1_555 1_555 1_555 yes N(3) C(2) C(4) 115.5(4) 1_555 1_555 1_555 yes N(3) C(2) C(6) 123.6(5) 1_555 1_555 1_555 yes C(4) C(2) C(6) 120.8(5) 1_555 1_555 1_555 yes N(4) C(3) C(1) 107.3(4) 1_555 1_555 1_555 yes N(4) C(3) C(7) 109.4(4) 1_555 1_555 1_555 yes N(4) C(3) C(8) 110.5(4) 1_555 1_555 1_555 yes C(1) C(3) C(7) 112.5(4) 1_555 1_555 1_555 yes C(1) C(3) C(8) 107.1(4) 1_555 1_555 1_555 yes C(7) C(3) C(8) 110.0(4) 1_555 1_555 1_555 yes N(5) C(4) C(2) 107.0(4) 1_555 1_555 1_555 yes N(5) C(4) C(9) 110.1(4) 1_555 1_555 1_555 yes N(5) C(4) C(10) 109.1(4) 1_555 1_555 1_555 yes C(2) C(4) C(9) 112.1(4) 1_555 1_555 1_555 yes C(2) C(4) C(10) 108.8(4) 1_555 1_555 1_555 yes C(9) C(4) C(10) 109.8(5) 1_555 1_555 1_555 yes C(1) C(5) H(4) 114(3) 1_555 1_555 1_555 no C(1) C(5) H(5) 115(3) 1_555 1_555 1_555 no C(1) C(5) H(6) 111(4) 1_555 1_555 1_555 no H(4) C(5) H(5) 100(4) 1_555 1_555 1_555 no H(4) C(5) H(6) 104(5) 1_555 1_555 1_555 no H(5) C(5) H(6) 109(5) 1_555 1_555 1_555 no C(2) C(6) H(7) 115(4) 1_555 1_555 1_555 no C(2) C(6) H(8) 109(3) 1_555 1_555 1_555 no C(2) C(6) H(9) 114(3) 1_555 1_555 1_555 no H(7) C(6) H(8) 100(4) 1_555 1_555 1_555 no H(7) C(6) H(9) 109(4) 1_555 1_555 1_555 no H(8) C(6) H(9) 106(4) 1_555 1_555 1_555 no C(3) C(7) H(10) 114(2) 1_555 1_555 1_555 no C(3) C(7) H(11) 111(2) 1_555 1_555 1_555 no C(3) C(7) H(12) 112(2) 1_555 1_555 1_555 no H(10) C(7) H(11) 103(3) 1_555 1_555 1_555 no H(10) C(7) H(12) 107(3) 1_555 1_555 1_555 no H(11) C(7) H(12) 107(3) 1_555 1_555 1_555 no C(3) C(8) H(13) 111(3) 1_555 1_555 1_555 no C(3) C(8) H(14) 111(3) 1_555 1_555 1_555 no C(3) C(8) H(15) 107(2) 1_555 1_555 1_555 no H(13) C(8) H(14) 110(4) 1_555 1_555 1_555 no H(13) C(8) H(15) 109(4) 1_555 1_555 1_555 no H(14) C(8) H(15) 107(3) 1_555 1_555 1_555 no C(4) C(9) H(16) 108(2) 1_555 1_555 1_555 no C(4) C(9) H(17) 104(3) 1_555 1_555 1_555 no C(4) C(9) H(18) 112(3) 1_555 1_555 1_555 no H(16) C(9) H(17) 115(4) 1_555 1_555 1_555 no H(16) C(9) H(18) 106(4) 1_555 1_555 1_555 no H(17) C(9) H(18) 110(4) 1_555 1_555 1_555 no C(4) C(10) H(19) 112(2) 1_555 1_555 1_555 no C(4) C(10) H(20) 104(2) 1_555 1_555 1_555 no C(4) C(10) H(21) 113(3) 1_555 1_555 1_555 no H(19) C(10) H(20) 110(3) 1_555 1_555 1_555 no H(19) C(10) H(21) 112(4) 1_555 1_555 1_555 no H(20) C(10) H(21) 103(4) 1_555 1_555 1_555 no N(4) C(11) C(13) 115.0(4) 1_555 1_555 1_555 yes N(4) C(11) H(22) 107(2) 1_555 1_555 1_555 no N(4) C(11) H(23) 106(2) 1_555 1_555 1_555 no C(13) C(11) H(22) 106(2) 1_555 1_555 1_555 no C(13) C(11) H(23) 110(2) 1_555 1_555 1_555 no H(22) C(11) H(23) 110(3) 1_555 1_555 1_555 no N(5) C(12) C(14) 110.2(4) 1_555 1_555 1_555 yes N(5) C(12) H(24) 108(2) 1_555 1_555 1_555 no N(5) C(12) H(25) 113(2) 1_555 1_555 1_555 no C(14) C(12) H(24) 111(2) 1_555 1_555 1_555 no C(14) C(12) H(25) 104(2) 1_555 1_555 1_555 no H(24) C(12) H(25) 109(3) 1_555 1_555 1_555 no C(11) C(13) C(14) 120.5(4) 1_555 1_555 1_555 yes C(11) C(13) H(26) 102(2) 1_555 1_555 1_555 no C(11) C(13) H(27) 110(3) 1_555 1_555 1_555 no C(14) C(13) H(26) 108(2) 1_555 1_555 1_555 no C(14) C(13) H(27) 116(3) 1_555 1_555 1_555 no H(26) C(13) H(27) 94(3) 1_555 1_555 1_555 no C(12) C(14) C(13) 121.6(5) 1_555 1_555 1_555 yes C(12) C(14) H(28) 106(2) 1_555 1_555 1_555 no C(12) C(14) H(29) 104(3) 1_555 1_555 1_555 no C(13) C(14) H(28) 108(2) 1_555 1_555 1_555 no C(13) C(14) H(29) 110(3) 1_555 1_555 1_555 no H(28) C(14) H(29) 102(4) 1_555 1_555 1_555 no C(16) C(15) C(20) 114.3(5) 1_555 1_555 1_555 yes C(16) C(15) B(1) 123.3(4) 1_555 1_555 1_555 yes C(20) C(15) B(1) 122.0(4) 1_555 1_555 1_555 yes C(15) C(16) C(17) 122.6(5) 1_555 1_555 1_555 yes C(15) C(16) H(32) 116(2) 1_555 1_555 1_555 no C(17) C(16) H(32) 120(2) 1_555 1_555 1_555 no C(16) C(17) C(18) 120.6(5) 1_555 1_555 1_555 yes C(16) C(17) H(33) 116(3) 1_555 1_555 1_555 no C(18) C(17) H(33) 122(3) 1_555 1_555 1_555 no C(17) C(18) C(19) 119.2(5) 1_555 1_555 1_555 yes C(17) C(18) H(34) 122(2) 1_555 1_555 1_555 no C(19) C(18) H(34) 117(2) 1_555 1_555 1_555 no C(18) C(19) C(20) 119.8(5) 1_555 1_555 1_555 yes C(18) C(19) H(35) 118(2) 1_555 1_555 1_555 no C(20) C(19) H(35) 121(2) 1_555 1_555 1_555 no C(15) C(20) C(19) 123.4(5) 1_555 1_555 1_555 yes C(15) C(20) H(36) 115(2) 1_555 1_555 1_555 no C(19) C(20) H(36) 121(2) 1_555 1_555 1_555 no C(22) C(21) C(26) 115.2(5) 1_555 1_555 1_555 yes C(22) C(21) B(1) 123.4(4) 1_555 1_555 1_555 yes C(26) C(21) B(1) 121.3(5) 1_555 1_555 1_555 yes C(21) C(22) C(23) 122.0(6) 1_555 1_555 1_555 yes C(21) C(22) H(37) 117(2) 1_555 1_555 1_555 no C(23) C(22) H(37) 120(2) 1_555 1_555 1_555 no C(22) C(23) C(24) 120.7(6) 1_555 1_555 1_555 yes C(22) C(23) H(38) 112(4) 1_555 1_555 1_555 no C(24) C(23) H(38) 126(4) 1_555 1_555 1_555 no C(23) C(24) C(25) 118.8(6) 1_555 1_555 1_555 yes C(23) C(24) H(39) 118(3) 1_555 1_555 1_555 no C(25) C(24) H(39) 122(3) 1_555 1_555 1_555 no C(24) C(25) C(26) 121.1(7) 1_555 1_555 1_555 yes C(24) C(25) H(40) 125(2) 1_555 1_555 1_555 no C(26) C(25) H(40) 112(2) 1_555 1_555 1_555 no C(21) C(26) C(25) 122.0(6) 1_555 1_555 1_555 yes C(21) C(26) H(41) 119(2) 1_555 1_555 1_555 no C(25) C(26) H(41) 117(2) 1_555 1_555 1_555 no C(28) C(27) C(32) 114.6(5) 1_555 1_555 1_555 yes C(28) C(27) B(1) 124.1(4) 1_555 1_555 1_555 yes C(32) C(27) B(1) 121.3(4) 1_555 1_555 1_555 yes C(27) C(28) C(29) 122.4(5) 1_555 1_555 1_555 yes C(27) C(28) H(42) 122(2) 1_555 1_555 1_555 no C(29) C(28) H(42) 114(2) 1_555 1_555 1_555 no C(28) C(29) C(30) 119.9(5) 1_555 1_555 1_555 yes C(28) C(29) H(43) 111(3) 1_555 1_555 1_555 no C(30) C(29) H(43) 128(3) 1_555 1_555 1_555 no C(29) C(30) C(31) 120.1(5) 1_555 1_555 1_555 yes C(29) C(30) H(44) 120(3) 1_555 1_555 1_555 no C(31) C(30) H(44) 118(3) 1_555 1_555 1_555 no C(30) C(31) C(32) 119.5(5) 1_555 1_555 1_555 yes C(30) C(31) H(45) 121(2) 1_555 1_555 1_555 no C(32) C(31) H(45) 119(2) 1_555 1_555 1_555 no C(27) C(32) C(31) 123.4(5) 1_555 1_555 1_555 yes C(27) C(32) H(46) 118(2) 1_555 1_555 1_555 no C(31) C(32) H(46) 118(2) 1_555 1_555 1_555 no C(34) C(33) C(38) 113.3(4) 1_555 1_555 1_555 yes C(34) C(33) B(1) 123.8(4) 1_555 1_555 1_555 yes C(38) C(33) B(1) 122.5(4) 1_555 1_555 1_555 yes C(33) C(34) C(35) 123.2(5) 1_555 1_555 1_555 yes C(33) C(34) H(47) 115(2) 1_555 1_555 1_555 no C(35) C(34) H(47) 121(2) 1_555 1_555 1_555 no C(34) C(35) C(36) 120.8(5) 1_555 1_555 1_555 yes C(34) C(35) H(48) 116(2) 1_555 1_555 1_555 no C(36) C(35) H(48) 122(2) 1_555 1_555 1_555 no C(35) C(36) C(37) 118.6(5) 1_555 1_555 1_555 yes C(35) C(36) H(49) 124(2) 1_555 1_555 1_555 no C(37) C(36) H(49) 116(2) 1_555 1_555 1_555 no C(36) C(37) C(38) 120.0(5) 1_555 1_555 1_555 yes C(36) C(37) H(50) 117(3) 1_555 1_555 1_555 no C(38) C(37) H(50) 122(3) 1_555 1_555 1_555 no C(33) C(38) C(37) 124.1(5) 1_555 1_555 1_555 yes C(33) C(38) H(51) 114(2) 1_555 1_555 1_555 no C(37) C(38) H(51) 120(2) 1_555 1_555 1_555 no C(15) B(1) C(21) 108.7(4) 1_555 1_555 1_555 yes C(15) B(1) C(27) 108.7(4) 1_555 1_555 1_555 yes C(15) B(1) C(33) 108.3(4) 1_555 1_555 1_555 yes C(21) B(1) C(27) 109.3(4) 1_555 1_555 1_555 yes C(21) B(1) C(33) 110.8(4) 1_555 1_555 1_555 yes C(27) B(1) C(33) 111.0(4) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(3) 2.699(4) 1_555 3_557 ? O(1) C(37) 3.188(6) 1_555 3_657 ? O(1) O(1) 3.314(7) 1_555 3_557 ? O(1) O(3) 3.426(4) 1_555 1_555 ? O(2) C(37) 3.444(6) 1_555 3_657 ? O(2) C(36) 3.461(6) 1_555 3_657 ? O(2) O(3) 3.503(4) 1_555 1_555 ? O(2) C(5) 3.551(8) 1_555 3_557 ? O(3) N(5) 2.902(5) 1_555 1_555 ? O(3) N(3) 2.909(5) 1_555 1_555 ? O(3) N(2) 2.960(5) 1_555 1_555 ? O(3) N(4) 3.115(5) 1_555 1_555 ? O(3) C(37) 3.260(6) 1_555 1_455 ? O(3) C(38) 3.353(6) 1_555 1_455 ? O(3) C(36) 3.400(6) 1_555 1_455 ? O(3) C(2) 3.586(6) 1_555 1_555 ? N(1) N(1) 3.027(8) 1_555 3_657 ? C(10) C(25) 3.565(9) 1_555 1_555 ? C(14) C(34) 3.546(8) 1_555 1_455 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #==END data_TcN-PentAO(3) #------------------------------------------------------------------------------ _audit_creation_date 'Wed Sep 17 14:51:54 1997' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 805.77 _chemical_formula_analytical ? _chemical_formula_sum 'C42 H59 B N5 O4 Tc ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.986(5) _cell_length_b 30.636(2) _cell_length_c 13.967(3) _cell_angle_alpha 90 _cell_angle_beta 95.24(3) _cell_angle_gamma 90 _cell_volume 4254(2) _cell_formula_units_Z 4 _cell_measurement_temperature 286.2 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 23.3 _cell_measurement_theta_max 24.7 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1704.00 _exptl_absorpt_coefficient_mu 0.380 _exptl_absorpt_correction_type '\DF (DIFABS; Walker & Stuart, 1983)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.910 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 286.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.93 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -3 -5 1 -8 -5 0 8 -5 _diffrn_reflns_number 10499 _reflns_number_total 9946 _reflns_number_observed 5599 _reflns_observed_criterion >4.0sigma(I) _diffrn_reflns_av_R_equivalents 3.58 _diffrn_reflns_av_sigmaI/netI 0.069 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05325 _diffrn_orient_matrix_UB_12 -0.00812 _diffrn_orient_matrix_UB_13 -0.05459 _diffrn_orient_matrix_UB_21 -0.08097 _diffrn_orient_matrix_UB_22 -0.01464 _diffrn_orient_matrix_UB_23 -0.03308 _diffrn_orient_matrix_UB_31 -0.02686 _diffrn_orient_matrix_UB_32 0.02802 _diffrn_orient_matrix_UB_33 -0.03309 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 168 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 236 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; B 0 4 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 20 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Tc 0 4 -1.439 0.759 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Tc1 0.41397(3) 0.086836(9) 0.85194(2) 0.03742(6) Uani d . 1.00 . O1 0.4113(3) 0.08652(9) 1.0692(2) 0.0613(8) Uani d . 1.00 . O2 0.3330(3) 0.01683(8) 0.9842(2) 0.0513(8) Uani d . 1.00 . O3 0.6219(2) 0.05081(8) 0.8990(2) 0.0461(7) Uani d . 1.00 . O4 -0.1729(3) 0.1087(1) 0.9231(3) 0.085(1) Uani d . 1.00 . N1 0.2723(3) 0.10876(10) 0.8145(2) 0.0508(9) Uani d . 1.00 . N2 0.4410(3) 0.11126(9) 0.9911(2) 0.0436(8) Uani d . 1.00 . N3 0.3499(3) 0.02543(9) 0.8908(2) 0.0442(8) Uani d . 1.00 . N4 0.5370(3) 0.14515(9) 0.8406(2) 0.0415(8) Uani d . 1.00 . N5 0.4353(3) 0.04791(9) 0.7249(2) 0.0464(8) Uani d . 1.00 . C1 0.4833(4) 0.1501(1) 1.0080(3) 0.048(1) Uani d . 1.00 . C2 0.3222(4) -0.0037(1) 0.8251(3) 0.055(1) Uani d . 1.00 . C3 0.5107(4) 0.1773(1) 0.9205(3) 0.046(1) Uani d . 1.00 . C4 0.3382(4) 0.0096(1) 0.7220(3) 0.056(1) Uani d . 1.00 . C5 0.4947(6) 0.1693(2) 1.1068(3) 0.082(2) Uani d . 1.00 . C6 0.2654(6) -0.0475(1) 0.8475(4) 0.087(2) Uani d . 1.00 . C7 0.6337(5) 0.2064(1) 0.9417(3) 0.067(1) Uani d . 1.00 . C8 0.3860(4) 0.2054(1) 0.8927(3) 0.061(1) Uani d . 1.00 . C9 0.3956(6) -0.0279(2) 0.6664(4) 0.090(2) Uani d . 1.00 . C10 0.1988(5) 0.0232(2) 0.6760(3) 0.078(2) Uani d . 1.00 . C11 0.5342(4) 0.1660(1) 0.7423(3) 0.055(1) Uani d . 1.00 . C12 0.4395(5) 0.0708(1) 0.6293(3) 0.063(1) Uani d . 1.00 . C13 0.6523(5) 0.1522(1) 0.6885(3) 0.068(1) Uani d . 1.00 . C14 0.5814(5) 0.0790(2) 0.6046(3) 0.072(2) Uani d . 1.00 . C15 0.6781(4) 0.1035(1) 0.6761(3) 0.064(1) Uani d . 1.00 . C16 0.1965(3) 0.1021(1) 0.3432(3) 0.0445(10) Uani d . 1.00 . C17 0.1610(4) 0.0723(1) 0.4113(3) 0.061(1) Uani d . 1.00 . C18 0.1462(6) 0.0278(2) 0.3924(4) 0.081(2) Uani d . 1.00 . C19 0.1692(5) 0.0120(1) 0.3038(4) 0.079(2) Uani d . 1.00 . C20 0.2040(5) 0.0399(2) 0.2339(4) 0.076(2) Uani d . 1.00 . C21 0.2176(4) 0.0840(1) 0.2540(3) 0.063(1) Uani d . 1.00 . C22 0.1525(4) 0.1696(1) 0.4628(3) 0.0446(10) Uani d . 1.00 . C23 0.2297(4) 0.1832(1) 0.5442(3) 0.059(1) Uani d . 1.00 . C24 0.1767(5) 0.1966(2) 0.6282(3) 0.075(2) Uani d . 1.00 . C25 0.0422(5) 0.1968(2) 0.6340(3) 0.078(2) Uani d . 1.00 . C26 -0.0386(5) 0.1836(2) 0.5561(4) 0.100(2) Uani d . 1.00 . C27 0.0161(5) 0.1702(2) 0.4731(3) 0.086(2) Uani d . 1.00 . C28 0.3746(3) 0.1684(1) 0.3661(2) 0.0398(9) Uani d . 1.00 . C29 0.4793(4) 0.1386(1) 0.3625(3) 0.051(1) Uani d . 1.00 . C30 0.6137(4) 0.1510(1) 0.3655(3) 0.064(1) Uani d . 1.00 . C31 0.6490(4) 0.1940(1) 0.3731(3) 0.062(1) Uani d . 1.00 . C32 0.5508(4) 0.2246(1) 0.3790(3) 0.059(1) Uani d . 1.00 . C33 0.4174(4) 0.2119(1) 0.3763(3) 0.051(1) Uani d . 1.00 . C34 0.1281(4) 0.1795(1) 0.2695(3) 0.047(1) Uani d . 1.00 . C35 0.1786(4) 0.2105(1) 0.2099(3) 0.058(1) Uani d . 1.00 . C36 0.1014(6) 0.2304(1) 0.1335(3) 0.076(2) Uani d . 1.00 . C37 -0.0299(7) 0.2209(2) 0.1156(4) 0.094(2) Uani d . 1.00 . C38 -0.0848(5) 0.1893(3) 0.1694(4) 0.119(3) Uani d . 1.00 . C39 -0.0057(5) 0.1686(2) 0.2435(4) 0.095(2) Uani d . 1.00 . C40 0.0138(8) 0.0678(4) 0.9635(9) 0.259(6) Uani d . 1.00 . C41 -0.0540(5) 0.1068(2) 0.9396(4) 0.087(2) Uani d . 1.00 . C42 0.0280(8) 0.1453(3) 0.9395(10) 0.283(6) Uani d . 1.00 . B1 0.2141(4) 0.1549(1) 0.3614(3) 0.042(1) Uani d . 1.00 . H1 0.3719 0.0569 1.0343 0.0696 Uiso calc . 1.00 . H2 0.6297 0.1350 0.8558 0.0696 Uiso calc . 1.00 . H3 0.5280 0.0354 0.7355 0.0696 Uiso calc . 1.00 . H4 0.4579 0.1981 1.1039 0.0981 Uiso calc . 1.00 . H5 0.5867 0.1708 1.1306 0.0981 Uiso calc . 1.00 . H6 0.4467 0.1519 1.1479 0.0981 Uiso calc . 1.00 . H7 0.1809 -0.0440 0.8748 0.1028 Uiso calc . 1.00 . H8 0.3252 -0.0628 0.8936 0.1028 Uiso calc . 1.00 . H9 0.2511 -0.0647 0.7911 0.1028 Uiso calc . 1.00 . H10 0.6527 0.2223 0.8852 0.0808 Uiso calc . 1.00 . H11 0.6203 0.2266 0.9914 0.0808 Uiso calc . 1.00 . H12 0.7115 0.1889 0.9614 0.0808 Uiso calc . 1.00 . H13 0.4052 0.2254 0.8437 0.0737 Uiso calc . 1.00 . H14 0.3628 0.2211 0.9474 0.0737 Uiso calc . 1.00 . H15 0.3132 0.1872 0.8696 0.0737 Uiso calc . 1.00 . H16 0.4108 -0.0190 0.6018 0.1057 Uiso calc . 1.00 . H17 0.4815 -0.0373 0.6970 0.1057 Uiso calc . 1.00 . H18 0.3371 -0.0524 0.6618 0.1057 Uiso calc . 1.00 . H19 0.2031 0.0326 0.6101 0.0939 Uiso calc . 1.00 . H20 0.1636 0.0475 0.7098 0.0939 Uiso calc . 1.00 . H21 0.1357 -0.0001 0.6757 0.0939 Uiso calc . 1.00 . H22 0.4522 0.1580 0.7049 0.0676 Uiso calc . 1.00 . H23 0.5340 0.1973 0.7491 0.0676 Uiso calc . 1.00 . H24 0.3948 0.0984 0.6317 0.0761 Uiso calc . 1.00 . H25 0.3927 0.0536 0.5798 0.0761 Uiso calc . 1.00 . H26 0.6411 0.1648 0.6250 0.0827 Uiso calc . 1.00 . H27 0.7320 0.1649 0.7212 0.0827 Uiso calc . 1.00 . H28 0.5767 0.0946 0.5453 0.0846 Uiso calc . 1.00 . H29 0.6200 0.0507 0.5940 0.0846 Uiso calc . 1.00 . H30 0.7674 0.0996 0.6574 0.0781 Uiso calc . 1.00 . H31 0.6742 0.0899 0.7378 0.0781 Uiso calc . 1.00 . H32 0.7095 0.0665 0.9179 0.0696 Uiso calc . 1.00 . H33 0.6321 0.0300 0.9569 0.0696 Uiso calc . 1.00 . H34 0.1442 0.0830 0.4751 0.0757 Uiso calc . 1.00 . H35 0.1206 0.0082 0.4426 0.0964 Uiso calc . 1.00 . H36 0.1614 -0.0190 0.2898 0.0965 Uiso calc . 1.00 . H37 0.2205 0.0297 0.1697 0.0922 Uiso calc . 1.00 . H38 0.2420 0.1040 0.2035 0.0768 Uiso calc . 1.00 . H39 0.3260 0.1834 0.5429 0.0698 Uiso calc . 1.00 . H40 0.2374 0.2070 0.6811 0.0871 Uiso calc . 1.00 . H41 0.0076 0.2054 0.6942 0.0907 Uiso calc . 1.00 . H42 -0.1362 0.1840 0.5584 0.1167 Uiso calc . 1.00 . H43 -0.0442 0.1605 0.4187 0.1032 Uiso calc . 1.00 . H44 0.4567 0.1078 0.3569 0.0613 Uiso calc . 1.00 . H45 0.6835 0.1291 0.3624 0.0773 Uiso calc . 1.00 . H46 0.7425 0.2027 0.3747 0.0735 Uiso calc . 1.00 . H47 0.5748 0.2553 0.3833 0.0707 Uiso calc . 1.00 . H48 0.3496 0.2342 0.3823 0.0627 Uiso calc . 1.00 . H49 0.2729 0.2187 0.2226 0.0719 Uiso calc . 1.00 . H50 0.1454 0.2510 0.0928 0.0873 Uiso calc . 1.00 . H51 -0.0828 0.2369 0.0669 0.1126 Uiso calc . 1.00 . H52 -0.1773 0.1811 0.1537 0.1386 Uiso calc . 1.00 . H53 -0.0459 0.1448 0.2784 0.1109 Uiso calc . 1.00 . H54 0.1080 0.0700 0.9725 0.2760 Uiso calc . 1.00 . H55 -0.0036 0.0465 0.9071 0.2760 Uiso calc . 1.00 . H56 -0.0196 0.0528 1.0157 0.2760 Uiso calc . 1.00 . H57 0.1197 0.1408 0.9498 0.2952 Uiso calc . 1.00 . H58 0.0145 0.1584 0.8705 0.2952 Uiso calc . 1.00 . H59 -0.0018 0.1680 0.9778 0.2952 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tc(1) 0.0436(1) 0.0325(1) 0.0363(1) 0.0007(2) 0.00384(10) 0.0037(1) O(1) 0.088(2) 0.059(2) 0.039(1) -0.012(2) 0.016(1) 0.006(1) O(2) 0.059(2) 0.042(1) 0.052(2) -0.005(1) 0.004(1) 0.015(1) O(3) 0.046(1) 0.043(1) 0.048(1) 0.001(1) -0.002(1) 0.011(1) O(4) 0.056(2) 0.066(2) 0.132(3) -0.009(2) 0.000(2) 0.020(2) N(1) 0.050(2) 0.047(2) 0.055(2) 0.007(1) 0.001(1) 0.007(1) N(2) 0.055(2) 0.043(2) 0.035(2) -0.003(1) 0.009(1) 0.001(1) N(3) 0.044(2) 0.036(2) 0.052(2) -0.002(1) 0.001(1) 0.008(1) N(4) 0.046(2) 0.034(1) 0.045(2) 0.002(1) 0.009(1) 0.007(1) N(5) 0.056(2) 0.045(2) 0.038(2) 0.003(1) -0.003(1) -0.003(1) C(1) 0.052(2) 0.044(2) 0.048(2) 0.001(2) 0.008(2) -0.005(2) C(2) 0.058(2) 0.040(2) 0.064(3) -0.006(2) -0.012(2) 0.002(2) C(3) 0.052(2) 0.032(2) 0.053(2) -0.003(2) 0.008(2) -0.002(2) C(4) 0.070(3) 0.043(2) 0.053(2) -0.002(2) -0.011(2) -0.006(2) C(5) 0.118(4) 0.071(3) 0.058(3) -0.016(3) 0.017(3) -0.023(2) C(6) 0.112(4) 0.050(3) 0.092(4) -0.031(3) -0.022(3) 0.006(2) C(7) 0.072(3) 0.047(2) 0.083(3) -0.015(2) 0.008(2) -0.007(2) C(8) 0.067(3) 0.045(2) 0.073(3) 0.010(2) 0.012(2) 0.000(2) C(9) 0.123(5) 0.061(3) 0.085(4) 0.002(3) 0.001(3) -0.027(3) C(10) 0.075(3) 0.091(4) 0.063(3) -0.013(3) -0.027(2) -0.001(3) C(11) 0.074(3) 0.042(2) 0.052(2) 0.008(2) 0.021(2) 0.017(2) C(12) 0.087(3) 0.068(3) 0.033(2) 0.007(2) -0.003(2) 0.001(2) C(13) 0.081(3) 0.059(3) 0.070(3) 0.005(2) 0.035(2) 0.015(2) C(14) 0.096(3) 0.079(3) 0.044(2) 0.017(3) 0.020(2) 0.009(2) C(15) 0.066(3) 0.070(3) 0.061(3) 0.011(2) 0.028(2) 0.013(2) C(16) 0.034(2) 0.048(2) 0.050(2) -0.001(1) -0.002(2) -0.001(2) C(17) 0.076(3) 0.053(2) 0.050(2) -0.009(2) -0.013(2) 0.004(2) C(18) 0.106(4) 0.054(3) 0.076(3) -0.016(3) -0.017(3) 0.011(2) C(19) 0.075(3) 0.045(2) 0.112(4) -0.003(2) -0.018(3) -0.010(3) C(20) 0.073(3) 0.070(3) 0.084(3) -0.001(3) 0.007(3) -0.030(3) C(21) 0.065(3) 0.058(2) 0.067(3) -0.007(2) 0.017(2) -0.016(2) C(22) 0.045(2) 0.046(2) 0.043(2) 0.004(2) 0.007(2) 0.005(2) C(23) 0.051(2) 0.081(3) 0.044(2) 0.009(2) 0.000(2) 0.002(2) C(24) 0.078(3) 0.107(4) 0.038(2) 0.012(3) -0.004(2) -0.001(2) C(25) 0.083(3) 0.107(4) 0.044(2) 0.019(3) 0.018(2) 0.002(3) C(26) 0.057(3) 0.176(6) 0.070(3) -0.001(3) 0.025(3) -0.013(4) C(27) 0.054(3) 0.149(5) 0.056(3) -0.017(3) 0.012(2) -0.027(3) C(28) 0.040(2) 0.044(2) 0.036(2) 0.004(1) 0.001(1) 0.000(1) C(29) 0.044(2) 0.042(2) 0.066(2) 0.002(2) 0.003(2) -0.001(2) C(30) 0.044(2) 0.054(2) 0.095(4) 0.009(2) 0.007(2) -0.008(2) C(31) 0.042(2) 0.062(3) 0.080(3) -0.006(2) 0.003(2) -0.009(2) C(32) 0.055(2) 0.050(2) 0.072(3) -0.007(2) 0.003(2) -0.006(2) C(33) 0.047(2) 0.044(2) 0.063(3) 0.004(2) 0.003(2) -0.008(2) C(34) 0.043(2) 0.054(2) 0.043(2) 0.007(2) 0.004(2) 0.000(2) C(35) 0.073(3) 0.052(2) 0.046(2) 0.004(2) -0.002(2) -0.002(2) C(36) 0.128(5) 0.049(2) 0.049(3) 0.008(3) -0.003(3) 0.005(2) C(37) 0.108(5) 0.113(5) 0.057(3) 0.052(4) -0.013(3) 0.006(3) C(38) 0.057(3) 0.223(8) 0.074(4) 0.022(4) -0.011(3) 0.040(5) C(39) 0.052(3) 0.164(6) 0.066(3) -0.006(3) -0.005(2) 0.047(3) C(40) 0.088(5) 0.34(1) 0.36(2) 0.098(8) 0.068(7) 0.22(1) C(41) 0.054(3) 0.119(5) 0.091(4) -0.011(3) 0.019(3) -0.024(3) C(42) 0.139(7) 0.220(10) 0.52(2) -0.117(7) 0.201(10) -0.26(1) B(1) 0.038(2) 0.044(2) 0.042(2) 0.002(2) 0.001(2) 0.001(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5599 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0337 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0360 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.300 _refine_ls_shift/esd_max 0.0030 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.22 _refine_diff_density_max 0.27 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tc(1) O(3) 2.390(3) 1_555 1_555 yes Tc(1) N(1) 1.610(3) 1_555 1_555 yes Tc(1) N(2) 2.077(3) 1_555 1_555 yes Tc(1) N(3) 2.075(3) 1_555 1_555 yes Tc(1) N(4) 2.182(3) 1_555 1_555 yes Tc(1) N(5) 2.164(3) 1_555 1_555 yes O(1) N(2) 1.382(3) 1_555 1_555 yes O(1) H(1) 1.085 1_555 1_555 no O(2) N(3) 1.357(4) 1_555 1_555 yes O(3) H(32) 1.012 1_555 1_555 no O(3) H(33) 1.027 1_555 1_555 no O(4) C(41) 1.190(6) 1_555 1_555 yes N(2) C(1) 1.278(4) 1_555 1_555 yes N(3) C(2) 1.292(4) 1_555 1_555 yes N(4) C(3) 1.528(4) 1_555 1_555 yes N(4) C(11) 1.512(4) 1_555 1_555 yes N(4) H(2) 0.982 1_555 1_555 no N(5) C(4) 1.520(5) 1_555 1_555 yes N(5) C(12) 1.512(5) 1_555 1_555 yes N(5) H(3) 1.000 1_555 1_555 no C(1) C(3) 1.523(5) 1_555 1_555 yes C(1) C(5) 1.496(5) 1_555 1_555 yes C(2) C(4) 1.518(6) 1_555 1_555 yes C(2) C(6) 1.500(5) 1_555 1_555 yes C(3) C(7) 1.525(5) 1_555 1_555 yes C(3) C(8) 1.535(5) 1_555 1_555 yes C(4) C(9) 1.528(6) 1_555 1_555 yes C(4) C(10) 1.536(6) 1_555 1_555 yes C(5) H(4) 0.955 1_555 1_555 no C(5) H(5) 0.949 1_555 1_555 no C(5) H(6) 0.945 1_555 1_555 no C(6) H(7) 0.963 1_555 1_555 no C(6) H(8) 0.961 1_555 1_555 no C(6) H(9) 0.947 1_555 1_555 no C(7) H(10) 0.960 1_555 1_555 no C(7) H(11) 0.949 1_555 1_555 no C(7) H(12) 0.963 1_555 1_555 no C(8) H(13) 0.950 1_555 1_555 no C(8) H(14) 0.949 1_555 1_555 no C(8) H(15) 0.950 1_555 1_555 no C(9) H(16) 0.969 1_555 1_555 no C(9) H(17) 0.966 1_555 1_555 no C(9) H(18) 0.950 1_555 1_555 no C(10) H(19) 0.970 1_555 1_555 no C(10) H(20) 0.966 1_555 1_555 no C(10) H(21) 0.950 1_555 1_555 no C(11) C(13) 1.516(6) 1_555 1_555 yes C(11) H(22) 0.962 1_555 1_555 no C(11) H(23) 0.964 1_555 1_555 no C(12) C(14) 1.510(6) 1_555 1_555 yes C(12) H(24) 0.960 1_555 1_555 no C(12) H(25) 0.956 1_555 1_555 no C(13) C(15) 1.528(6) 1_555 1_555 yes C(13) H(26) 0.963 1_555 1_555 no C(13) H(27) 0.963 1_555 1_555 no C(14) C(15) 1.521(6) 1_555 1_555 yes C(14) H(28) 0.953 1_555 1_555 no C(14) H(29) 0.967 1_555 1_555 no C(15) H(30) 0.960 1_555 1_555 no C(15) H(31) 0.960 1_555 1_555 no C(16) C(17) 1.388(5) 1_555 1_555 yes C(16) C(21) 1.397(5) 1_555 1_555 yes C(16) B(1) 1.644(5) 1_555 1_555 yes C(17) C(18) 1.394(6) 1_555 1_555 yes C(17) H(34) 0.979 1_555 1_555 no C(18) C(19) 1.369(7) 1_555 1_555 yes C(18) H(35) 0.974 1_555 1_555 no C(19) C(20) 1.365(7) 1_555 1_555 yes C(19) H(36) 0.972 1_555 1_555 no C(20) C(21) 1.385(6) 1_555 1_555 yes C(20) H(37) 0.977 1_555 1_555 no C(21) H(38) 0.981 1_555 1_555 no C(22) C(23) 1.378(5) 1_555 1_555 yes C(22) C(27) 1.383(6) 1_555 1_555 yes C(22) B(1) 1.657(5) 1_555 1_555 yes C(23) C(24) 1.392(6) 1_555 1_555 yes C(23) H(39) 0.963 1_555 1_555 no C(24) C(25) 1.354(6) 1_555 1_555 yes C(24) H(40) 0.965 1_555 1_555 no C(25) C(26) 1.356(7) 1_555 1_555 yes C(25) H(41) 0.973 1_555 1_555 no C(26) C(27) 1.389(6) 1_555 1_555 yes C(26) H(42) 0.978 1_555 1_555 no C(27) H(43) 0.971 1_555 1_555 no C(28) C(29) 1.392(5) 1_555 1_555 yes C(28) C(33) 1.403(5) 1_555 1_555 yes C(28) B(1) 1.650(5) 1_555 1_555 yes C(29) C(30) 1.392(5) 1_555 1_555 yes C(29) H(44) 0.971 1_555 1_555 no C(30) C(31) 1.367(6) 1_555 1_555 yes C(30) H(45) 0.971 1_555 1_555 no C(31) C(32) 1.365(6) 1_555 1_555 yes C(31) H(46) 0.968 1_555 1_555 no C(32) C(33) 1.386(5) 1_555 1_555 yes C(32) H(47) 0.970 1_555 1_555 no C(33) H(48) 0.971 1_555 1_555 no C(34) C(35) 1.388(5) 1_555 1_555 yes C(34) C(39) 1.393(6) 1_555 1_555 yes C(34) B(1) 1.657(5) 1_555 1_555 yes C(35) C(36) 1.399(6) 1_555 1_555 yes C(35) H(49) 0.975 1_555 1_555 no C(36) C(37) 1.344(8) 1_555 1_555 yes C(36) H(50) 0.979 1_555 1_555 no C(37) C(38) 1.370(8) 1_555 1_555 yes C(37) H(51) 0.956 1_555 1_555 no C(38) C(39) 1.395(7) 1_555 1_555 yes C(38) H(52) 0.964 1_555 1_555 no C(39) H(53) 0.984 1_555 1_555 no C(40) C(41) 1.40(1) 1_555 1_555 yes C(40) H(54) 0.940 1_555 1_555 no C(40) H(55) 1.025 1_555 1_555 no C(40) H(56) 0.949 1_555 1_555 no C(41) C(42) 1.438(9) 1_555 1_555 yes C(42) H(57) 0.924 1_555 1_555 no C(42) H(58) 1.040 1_555 1_555 no C(42) H(59) 0.943 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(3) Tc(1) N(1) 176.2(1) 1_555 1_555 1_555 yes O(3) Tc(1) N(2) 82.73(10) 1_555 1_555 1_555 yes O(3) Tc(1) N(3) 77.89(10) 1_555 1_555 1_555 yes O(3) Tc(1) N(4) 85.27(9) 1_555 1_555 1_555 yes O(3) Tc(1) N(5) 79.81(10) 1_555 1_555 1_555 yes N(1) Tc(1) N(2) 100.9(1) 1_555 1_555 1_555 yes N(1) Tc(1) N(3) 100.4(1) 1_555 1_555 1_555 yes N(1) Tc(1) N(4) 96.8(1) 1_555 1_555 1_555 yes N(1) Tc(1) N(5) 96.5(1) 1_555 1_555 1_555 yes N(2) Tc(1) N(3) 95.7(1) 1_555 1_555 1_555 yes N(2) Tc(1) N(4) 75.4(1) 1_555 1_555 1_555 yes N(2) Tc(1) N(5) 162.1(1) 1_555 1_555 1_555 yes N(3) Tc(1) N(4) 161.9(1) 1_555 1_555 1_555 yes N(3) Tc(1) N(5) 76.7(1) 1_555 1_555 1_555 yes N(4) Tc(1) N(5) 107.1(1) 1_555 1_555 1_555 yes N(2) O(1) H(1) 101.5(2) 1_555 1_555 1_555 no Tc(1) O(3) H(32) 124.2(2) 1_555 1_555 1_555 no Tc(1) O(3) H(33) 121.6(2) 1_555 1_555 1_555 no H(32) O(3) H(33) 93.9(2) 1_555 1_555 1_555 no Tc(1) N(2) O(1) 121.5(2) 1_555 1_555 1_555 yes Tc(1) N(2) C(1) 121.4(2) 1_555 1_555 1_555 yes O(1) N(2) C(1) 117.2(3) 1_555 1_555 1_555 yes Tc(1) N(3) O(2) 119.7(2) 1_555 1_555 1_555 yes Tc(1) N(3) C(2) 119.4(3) 1_555 1_555 1_555 yes O(2) N(3) C(2) 120.8(3) 1_555 1_555 1_555 yes Tc(1) N(4) C(3) 109.8(2) 1_555 1_555 1_555 yes Tc(1) N(4) C(11) 116.7(2) 1_555 1_555 1_555 yes Tc(1) N(4) H(2) 104.5(2) 1_555 1_555 1_555 no C(3) N(4) C(11) 113.6(3) 1_555 1_555 1_555 yes C(3) N(4) H(2) 105.5(3) 1_555 1_555 1_555 no C(11) N(4) H(2) 105.6(3) 1_555 1_555 1_555 no Tc(1) N(5) C(4) 109.7(2) 1_555 1_555 1_555 yes Tc(1) N(5) C(12) 118.8(2) 1_555 1_555 1_555 yes Tc(1) N(5) H(3) 104.5(2) 1_555 1_555 1_555 no C(4) N(5) C(12) 113.8(3) 1_555 1_555 1_555 yes C(4) N(5) H(3) 106.6(3) 1_555 1_555 1_555 no C(12) N(5) H(3) 102.0(3) 1_555 1_555 1_555 no N(2) C(1) C(3) 116.2(3) 1_555 1_555 1_555 yes N(2) C(1) C(5) 122.2(4) 1_555 1_555 1_555 yes C(3) C(1) C(5) 121.5(3) 1_555 1_555 1_555 yes N(3) C(2) C(4) 117.0(3) 1_555 1_555 1_555 yes N(3) C(2) C(6) 122.0(4) 1_555 1_555 1_555 yes C(4) C(2) C(6) 120.8(4) 1_555 1_555 1_555 yes N(4) C(3) C(1) 106.8(3) 1_555 1_555 1_555 yes N(4) C(3) C(7) 109.2(3) 1_555 1_555 1_555 yes N(4) C(3) C(8) 111.5(3) 1_555 1_555 1_555 yes C(1) C(3) C(7) 111.4(3) 1_555 1_555 1_555 yes C(1) C(3) C(8) 108.0(3) 1_555 1_555 1_555 yes C(7) C(3) C(8) 109.9(3) 1_555 1_555 1_555 yes N(5) C(4) C(2) 107.7(3) 1_555 1_555 1_555 yes N(5) C(4) C(9) 109.1(4) 1_555 1_555 1_555 yes N(5) C(4) C(10) 110.7(3) 1_555 1_555 1_555 yes C(2) C(4) C(9) 110.9(4) 1_555 1_555 1_555 yes C(2) C(4) C(10) 107.4(4) 1_555 1_555 1_555 yes C(9) C(4) C(10) 111.0(4) 1_555 1_555 1_555 yes C(1) C(5) H(4) 109.1(4) 1_555 1_555 1_555 no C(1) C(5) H(5) 109.3(4) 1_555 1_555 1_555 no C(1) C(5) H(6) 109.8(4) 1_555 1_555 1_555 no H(4) C(5) H(5) 109.1(5) 1_555 1_555 1_555 no H(4) C(5) H(6) 109.5(5) 1_555 1_555 1_555 no H(5) C(5) H(6) 110.0(5) 1_555 1_555 1_555 no C(2) C(6) H(7) 110.3(4) 1_555 1_555 1_555 no C(2) C(6) H(8) 110.8(4) 1_555 1_555 1_555 no C(2) C(6) H(9) 110.8(5) 1_555 1_555 1_555 no H(7) C(6) H(8) 107.5(5) 1_555 1_555 1_555 no H(7) C(6) H(9) 108.6(5) 1_555 1_555 1_555 no H(8) C(6) H(9) 108.8(5) 1_555 1_555 1_555 no C(3) C(7) H(10) 110.7(4) 1_555 1_555 1_555 no C(3) C(7) H(11) 111.1(4) 1_555 1_555 1_555 no C(3) C(7) H(12) 110.2(4) 1_555 1_555 1_555 no H(10) C(7) H(11) 108.8(4) 1_555 1_555 1_555 no H(10) C(7) H(12) 107.6(4) 1_555 1_555 1_555 no H(11) C(7) H(12) 108.5(4) 1_555 1_555 1_555 no C(3) C(8) H(13) 109.4(4) 1_555 1_555 1_555 no C(3) C(8) H(14) 109.4(4) 1_555 1_555 1_555 no C(3) C(8) H(15) 109.5(3) 1_555 1_555 1_555 no H(13) C(8) H(14) 109.5(4) 1_555 1_555 1_555 no H(13) C(8) H(15) 109.5(4) 1_555 1_555 1_555 no H(14) C(8) H(15) 109.6(4) 1_555 1_555 1_555 no C(4) C(9) H(16) 111.0(4) 1_555 1_555 1_555 no C(4) C(9) H(17) 111.0(4) 1_555 1_555 1_555 no C(4) C(9) H(18) 111.9(5) 1_555 1_555 1_555 no H(16) C(9) H(17) 106.6(6) 1_555 1_555 1_555 no H(16) C(9) H(18) 107.9(5) 1_555 1_555 1_555 no H(17) C(9) H(18) 108.2(5) 1_555 1_555 1_555 no C(4) C(10) H(19) 111.1(5) 1_555 1_555 1_555 no C(4) C(10) H(20) 111.1(4) 1_555 1_555 1_555 no C(4) C(10) H(21) 112.0(4) 1_555 1_555 1_555 no H(19) C(10) H(20) 106.5(5) 1_555 1_555 1_555 no H(19) C(10) H(21) 107.8(4) 1_555 1_555 1_555 no H(20) C(10) H(21) 108.1(5) 1_555 1_555 1_555 no N(4) C(11) C(13) 112.5(3) 1_555 1_555 1_555 yes N(4) C(11) H(22) 109.2(3) 1_555 1_555 1_555 no N(4) C(11) H(23) 109.4(3) 1_555 1_555 1_555 no C(13) C(11) H(22) 108.7(4) 1_555 1_555 1_555 no C(13) C(11) H(23) 109.6(3) 1_555 1_555 1_555 no H(22) C(11) H(23) 107.3(4) 1_555 1_555 1_555 no N(5) C(12) C(14) 112.4(3) 1_555 1_555 1_555 yes N(5) C(12) H(24) 109.2(3) 1_555 1_555 1_555 no N(5) C(12) H(25) 109.5(4) 1_555 1_555 1_555 no C(14) C(12) H(24) 108.0(4) 1_555 1_555 1_555 no C(14) C(12) H(25) 109.5(4) 1_555 1_555 1_555 no H(24) C(12) H(25) 108.1(4) 1_555 1_555 1_555 no C(11) C(13) C(15) 118.4(3) 1_555 1_555 1_555 yes C(11) C(13) H(26) 108.4(4) 1_555 1_555 1_555 no C(11) C(13) H(27) 107.4(4) 1_555 1_555 1_555 no C(15) C(13) H(26) 107.1(4) 1_555 1_555 1_555 no C(15) C(13) H(27) 107.9(4) 1_555 1_555 1_555 no H(26) C(13) H(27) 107.3(4) 1_555 1_555 1_555 no C(12) C(14) C(15) 119.0(3) 1_555 1_555 1_555 yes C(12) C(14) H(28) 108.0(4) 1_555 1_555 1_555 no C(12) C(14) H(29) 106.2(4) 1_555 1_555 1_555 no C(15) C(14) H(28) 107.6(4) 1_555 1_555 1_555 no C(15) C(14) H(29) 107.8(4) 1_555 1_555 1_555 no H(28) C(14) H(29) 107.8(4) 1_555 1_555 1_555 no C(13) C(15) C(14) 116.9(4) 1_555 1_555 1_555 yes C(13) C(15) H(30) 108.8(4) 1_555 1_555 1_555 no C(13) C(15) H(31) 107.5(4) 1_555 1_555 1_555 no C(14) C(15) H(30) 108.1(4) 1_555 1_555 1_555 no C(14) C(15) H(31) 107.5(4) 1_555 1_555 1_555 no H(30) C(15) H(31) 107.8(4) 1_555 1_555 1_555 no C(17) C(16) C(21) 114.8(4) 1_555 1_555 1_555 yes C(17) C(16) B(1) 124.9(3) 1_555 1_555 1_555 yes C(21) C(16) B(1) 120.4(3) 1_555 1_555 1_555 yes C(16) C(17) C(18) 122.9(4) 1_555 1_555 1_555 yes C(16) C(17) H(34) 118.7(4) 1_555 1_555 1_555 no C(18) C(17) H(34) 118.4(4) 1_555 1_555 1_555 no C(17) C(18) C(19) 119.5(4) 1_555 1_555 1_555 yes C(17) C(18) H(35) 119.8(5) 1_555 1_555 1_555 no C(19) C(18) H(35) 120.7(5) 1_555 1_555 1_555 no C(18) C(19) C(20) 120.0(4) 1_555 1_555 1_555 yes C(18) C(19) H(36) 120.7(6) 1_555 1_555 1_555 no C(20) C(19) H(36) 119.3(6) 1_555 1_555 1_555 no C(19) C(20) C(21) 119.5(4) 1_555 1_555 1_555 yes C(19) C(20) H(37) 122.1(5) 1_555 1_555 1_555 no C(21) C(20) H(37) 118.4(5) 1_555 1_555 1_555 no C(16) C(21) C(20) 123.2(4) 1_555 1_555 1_555 yes C(16) C(21) H(38) 117.4(4) 1_555 1_555 1_555 no C(20) C(21) H(38) 119.3(4) 1_555 1_555 1_555 no C(23) C(22) C(27) 113.1(4) 1_555 1_555 1_555 yes C(23) C(22) B(1) 124.4(3) 1_555 1_555 1_555 yes C(27) C(22) B(1) 122.5(3) 1_555 1_555 1_555 yes C(22) C(23) C(24) 123.9(4) 1_555 1_555 1_555 yes C(22) C(23) H(39) 118.0(4) 1_555 1_555 1_555 no C(24) C(23) H(39) 118.0(4) 1_555 1_555 1_555 no C(23) C(24) C(25) 120.5(4) 1_555 1_555 1_555 yes C(23) C(24) H(40) 118.8(5) 1_555 1_555 1_555 no C(25) C(24) H(40) 120.7(5) 1_555 1_555 1_555 no C(24) C(25) C(26) 118.2(4) 1_555 1_555 1_555 yes C(24) C(25) H(41) 119.0(5) 1_555 1_555 1_555 no C(26) C(25) H(41) 122.8(5) 1_555 1_555 1_555 no C(25) C(26) C(27) 120.5(5) 1_555 1_555 1_555 yes C(25) C(26) H(42) 119.5(5) 1_555 1_555 1_555 no C(27) C(26) H(42) 120.0(5) 1_555 1_555 1_555 no C(22) C(27) C(26) 123.8(4) 1_555 1_555 1_555 yes C(22) C(27) H(43) 117.4(4) 1_555 1_555 1_555 no C(26) C(27) H(43) 118.7(5) 1_555 1_555 1_555 no C(29) C(28) C(33) 113.8(3) 1_555 1_555 1_555 yes C(29) C(28) B(1) 124.4(3) 1_555 1_555 1_555 yes C(33) C(28) B(1) 121.8(3) 1_555 1_555 1_555 yes C(28) C(29) C(30) 123.1(3) 1_555 1_555 1_555 yes C(28) C(29) H(44) 118.0(4) 1_555 1_555 1_555 no C(30) C(29) H(44) 118.9(4) 1_555 1_555 1_555 no C(29) C(30) C(31) 120.5(4) 1_555 1_555 1_555 yes C(29) C(30) H(45) 120.3(4) 1_555 1_555 1_555 no C(31) C(30) H(45) 119.2(4) 1_555 1_555 1_555 no C(30) C(31) C(32) 119.0(4) 1_555 1_555 1_555 yes C(30) C(31) H(46) 120.4(4) 1_555 1_555 1_555 no C(32) C(31) H(46) 120.5(4) 1_555 1_555 1_555 no C(31) C(32) C(33) 119.9(4) 1_555 1_555 1_555 yes C(31) C(32) H(47) 119.6(4) 1_555 1_555 1_555 no C(33) C(32) H(47) 120.5(4) 1_555 1_555 1_555 no C(28) C(33) C(32) 123.6(3) 1_555 1_555 1_555 yes C(28) C(33) H(48) 118.0(4) 1_555 1_555 1_555 no C(32) C(33) H(48) 118.4(4) 1_555 1_555 1_555 no C(35) C(34) C(39) 113.5(4) 1_555 1_555 1_555 yes C(35) C(34) B(1) 125.7(3) 1_555 1_555 1_555 yes C(39) C(34) B(1) 120.7(4) 1_555 1_555 1_555 yes C(34) C(35) C(36) 123.5(4) 1_555 1_555 1_555 yes C(34) C(35) H(49) 117.7(4) 1_555 1_555 1_555 no C(36) C(35) H(49) 118.8(4) 1_555 1_555 1_555 no C(35) C(36) C(37) 120.5(5) 1_555 1_555 1_555 yes C(35) C(36) H(50) 118.7(6) 1_555 1_555 1_555 no C(37) C(36) H(50) 120.8(5) 1_555 1_555 1_555 no C(36) C(37) C(38) 118.9(5) 1_555 1_555 1_555 yes C(36) C(37) H(51) 119.2(7) 1_555 1_555 1_555 no C(38) C(37) H(51) 121.9(7) 1_555 1_555 1_555 no C(37) C(38) C(39) 120.0(5) 1_555 1_555 1_555 yes C(37) C(38) H(52) 118.9(6) 1_555 1_555 1_555 no C(39) C(38) H(52) 121.0(7) 1_555 1_555 1_555 no C(34) C(39) C(38) 123.4(5) 1_555 1_555 1_555 yes C(34) C(39) H(53) 118.2(4) 1_555 1_555 1_555 no C(38) C(39) H(53) 118.5(5) 1_555 1_555 1_555 no C(41) C(40) H(54) 115(1) 1_555 1_555 1_555 no C(41) C(40) H(55) 108.4(8) 1_555 1_555 1_555 no C(41) C(40) H(56) 113.7(9) 1_555 1_555 1_555 no H(54) C(40) H(55) 104(1) 1_555 1_555 1_555 no H(54) C(40) H(56) 110.5(9) 1_555 1_555 1_555 no H(55) C(40) H(56) 103(1) 1_555 1_555 1_555 no O(4) C(41) C(40) 122.8(7) 1_555 1_555 1_555 yes O(4) C(41) C(42) 121.2(7) 1_555 1_555 1_555 yes C(40) C(41) C(42) 116.0(7) 1_555 1_555 1_555 yes C(41) C(42) H(57) 115(1) 1_555 1_555 1_555 no C(41) C(42) H(58) 107.0(8) 1_555 1_555 1_555 no C(41) C(42) H(59) 113.3(7) 1_555 1_555 1_555 no H(57) C(42) H(58) 104.2(9) 1_555 1_555 1_555 no H(57) C(42) H(59) 112.4(9) 1_555 1_555 1_555 no H(58) C(42) H(59) 102(1) 1_555 1_555 1_555 no C(16) B(1) C(22) 110.9(3) 1_555 1_555 1_555 yes C(16) B(1) C(28) 110.0(3) 1_555 1_555 1_555 yes C(16) B(1) C(34) 106.6(3) 1_555 1_555 1_555 yes C(22) B(1) C(28) 109.4(3) 1_555 1_555 1_555 yes C(22) B(1) C(34) 109.4(3) 1_555 1_555 1_555 yes C(28) B(1) C(34) 110.5(3) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(21) 3.364(5) 1_555 1_556 ? O(1) C(20) 3.534(6) 1_555 1_556 ? O(1) C(6) 3.538(6) 1_555 3_657 ? O(2) O(3) 2.650(3) 1_555 3_657 ? O(2) O(2) 3.481(5) 1_555 3_657 ? O(2) C(40) 3.537(8) 1_555 1_555 ? O(3) O(4) 2.707(4) 1_555 1_655 ? O(4) N(4) 3.219(4) 1_555 1_455 ? O(4) C(7) 3.585(6) 1_555 1_455 ? N(1) C(42) 3.321(8) 1_555 1_555 ? C(37) C(42) 3.465(9) 1_555 1_554 ? #------------------------------------------------------------------------------